Methanol → HCID 23092590、化合物

To a stirred solution of 1-(2-amino-1,3-thiazol-4-yl)ethanone (10 g, 70.33 mmol, 1 eq.) in 100 ml dry THF cooled to 5° C., was added LiBH4 (2M in THF, 38.7 ml, 77.36 mmol, 1.1 eq.) followed by MeOH (3.2 ml, 78 mmol, 1.11 eq.). The reaction was allowed to warm to r.t. and was stirred for further 18 hrs. The solvent was evaporated and the residue was partitioned between 250 ml EtOAc/250 ml water. Stirring was allowed for 10 mins. And the brown solid was filtered. The organic layer was separated, washed with brine, dried with MgSO4 and evaporated to give viscous orange oil. The residue was purified by chromatography on silica gel to give 1-(2-amino-1,3-thiazol-4-yl)ethanol (2 g, 19% yield) as a white solid.

1. customThe solvent was evaporated
2. customthe residue was partitioned between 250 ml EtOAc/250 ml water
3. stirringStirring
4. waitwas allowed for 10 mins
5. filtrationAnd the brown solid was filtered
6. customThe organic layer was separated
7. washwashed with brine
8. dry with materialdried with MgSO4
9. customevaporated
10. customto give viscous orange oil
11. customThe residue was purified by chromatography on silica gel

ORDレコード

ord-35cf0f6212a0444e8c8de6bba0dd6002

出典データセット

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08557849B2